CN113820434B - Method for identifying maturity of acacia honey - Google Patents
Method for identifying maturity of acacia honey Download PDFInfo
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- CN113820434B CN113820434B CN202111390505.XA CN202111390505A CN113820434B CN 113820434 B CN113820434 B CN 113820434B CN 202111390505 A CN202111390505 A CN 202111390505A CN 113820434 B CN113820434 B CN 113820434B
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Abstract
The invention relates to the technical field of food detection, in particular to a method for identifying maturity of acacia honey. The method for identifying the maturity of the acacia honey provided by the invention comprises the steps of detecting the acacia honey sample by taking turanose as a characteristic marker, judging the acacia honey sample to be mature acacia honey if the content of turanose in the acacia honey sample is more than or equal to 0.5%, judging the acacia honey sample to be semi-mature acacia honey if the content of turanose in the acacia honey sample is more than or equal to 0.3% and less than 0.5%, and judging the acacia honey sample to be immature acacia honey if the content of turanose in the acacia honey sample is less than 0.3%. The method has the characteristics of simple operation, high efficiency, low cost and the like, has reliable and stable detection results and high judgment degree, can be used for quality evaluation and grading of the acacia honey, and is convenient to popularize and apply.
Description
Technical Field
The invention relates to the technical field of food detection, in particular to a method for identifying maturity of acacia honey.
Background
The acacia honey is prepared by collecting the nectar of acacia by bees. The acacia honey is water white in color, soft in taste, sweet but not greasy, has unique sophora flower fragrance, belongs to a high-quality high-end honey variety, and has a market value obviously higher than that of other honey. The maturation process of the acacia honey starts from the completion of the work of collecting the nectar by the bees, the collected bees take the acacia nectar into the honey sacs and bring the acacia nectar back to the honeycomb, and brewing of the acacia honey in the honeycomb is started. During the collection process, the collected bees secrete invertase and amylase to mix into the nectar, and after the nectar is homed, honey juice is spitted out and distributed to the housework bees. The domestic bees suck honey juice into the honey sacs, and repeatedly suck and shrink by using the beaks of the domestic bees, and various enzymes are continuously added into the domestic bees during the repeated process to realize component conversion. Continuously vibrating wings of the domestic bees during huff and puff and transformation to accelerate water evaporation, and when the water content of honey in the honey spleens is reduced to about 20%, sealing the honey spleens with beewax by the bees, and then basically maturing the acacia honey. In general, the maturation process of acacia honey takes at least 7 days, and the sealing of honey spleens reaches 75% and above. Thus, acacia honey brewed in a honeycomb for at least 7 days and honey spleens capped at 75% and above is generally considered mature acacia honey.
However, acacia flowers have a short flowering period, and in order to maximize the yield, more than 1 to 3 days of acacia honey is usually collected manually, and the water content is reduced to 21% or less by manual concentration, thereby obtaining immature acacia honey. The physicochemical indexes of the immature acacia honey all meet the requirements of the physicochemical indexes of national standard acacia honey, so that the immature acacia honey cannot be effectively distinguished from the naturally mature acacia honey, and whether the acacia honey is mature or not and how the acacia honey is mature are difficult to distinguish. The values of the acacia honey with different maturity in the current market are different, and in order to pursue high value, some enterprises sell the immature or incompletely mature acacia honey as the mature acacia honey, so that the market order of the honey is seriously disturbed. Therefore, it is necessary to develop a stable and reliable index for determining the maturity of acacia honey, so as to distinguish different qualities of acacia honey and ensure the quality and value of acacia honey.
Disclosure of Invention
The invention aims to provide a method for identifying the maturity of acacia honey by using turanose as a characteristic marker.
The material composition of honey can be changed in the maturation process, but not high-content chemical components in the honey can generate characteristic content change in the maturation process, and the content change of many components has no following rule and is difficult to be used as a characteristic marker of the mature honey. The honey adulteration and the honey maturity are two different evaluation modes of honey, and compared with adulteration, the maturity evaluation can well realize product grading, namely under the condition of not relating to adulteration, the product is divided into different grades according to the different maturity, so that different values of the product are realized. The identification and evaluation of the maturity have an important supporting role in realizing the high-quality and high-price of the honey. According to the invention, in the research on the maturation process of acacia honey, the content change of turanose in the maturation process of acacia honey is obviously related to the brewing time and the sealing cover in a nest, and the turanose can be used as a characteristic marker for identifying mature acacia honey and immature acacia honey. Further, the content change characteristics of the turanose in the acacia honey with different maturity are very stable through detecting the acacia honey with large sample amount of different years, different sources and different maturity, and the turanose is expensive and is difficult to be artificially added into the acacia honey, so that the turanose is suitable to be used as a characteristic marker of the acacia honey maturity and is used for identifying mature acacia honey and immature acacia honey.
Based on the above findings, the present invention provides the following technical solutions:
in a first aspect, the present invention provides the use of turanose as a marker characteristic of mature acacia honey.
In a second aspect, the invention provides the use of turanose for identifying the maturity of acacia honey.
In a third aspect, the invention provides the use of turanose for the identification of mature acacia honey from immature acacia honey.
In a fourth aspect, the invention provides a method for identifying the maturity of acacia honey, which comprises the following steps: detecting the acacia honey sample by taking the turanose as a characteristic marker, if the content of the turanose in the acacia honey sample to be identified is more than or equal to 0.5%, judging the acacia honey sample to be identified as mature acacia honey, if the content of the turanose in the acacia honey sample to be identified is more than or equal to 0.3% and less than 0.5%, judging the acacia honey sample to be identified as semi-mature acacia honey, and if the content of the turanose in the acacia honey sample to be identified is less than 0.3%, judging the acacia honey sample to be identified as immature acacia honey.
Wherein the mature acacia honey is brewed in honeycomb for at least 7 days, and the sealing rate of the honey comb is more than or equal to 75 percent;
the semi-immature acacia honey is brewed in a honeycomb for more than 3 days and less than or equal to 5 days, and the sealing rate of the honey comb is 30-70%;
the immature honey is brewed in honeycomb for 0-3 days, and the sealing cover of honey comb is less than or equal to 10%.
Preferably, the identification method adopts a high performance liquid chromatography evaporative light scattering detector to detect the acacia honey sample.
Specifically, a standard curve is prepared from the linear relationship between the content of turanose and the peak area, and the content is calculated from the standard curve and the peak area of turanose detected in the acacia honey sample.
In the present invention, the content of turanose is the mass percentage content relative to the acacia honey sample.
The identification method comprises the following steps: detecting the acacia honey sample to be identified by adopting a high performance liquid chromatography evaporative light scattering detector, wherein the obtained spectrogram contains a characteristic peak corresponding to turanose, and the content of the characteristic peak is more than or equal to 0.5%, and then judging that the acacia honey sample is mature acacia honey.
Preferably, the liquid phase conditions detected by the high performance liquid chromatography evaporative light scattering detector are as follows: a Hi-Plex Pb, USP L19 column is used, the column temperature being 68-72 deg.C (preferably 70 deg.C).
The Hi-Plex Pb, USP L19 chromatographic column may be specifically Agilent Hi-Plex Pb, USP L19, 4.0X 250 mm.
The liquid chromatogram takes water as a mobile phase, and the elution method is isocratic elution.
When the above liquid phase conditions are employed, the flow rate of the mobile phase is preferably 0.5 to 0.7mL/min (more preferably 0.6 mL/min), and the amount of the sample is preferably 45 to 55. mu.L (more preferably 50. mu.L).
Preferably, the evaporative light scattering detector conditions detected by the high performance liquid chromatography evaporative light scattering detector are as follows: the atomization temperature was 90 ℃, the evaporation temperature was 60 ℃ and the carrier gas flow rate was 1.2 SLM.
Before the detection of the high performance liquid chromatography evaporative light scattering detector, the method also comprises the step of pretreating the acacia honey sample, wherein the pretreatment comprises the following steps: dissolving the acacia honey sample in water, and filtering.
Specifically, the acacia honey sample is dissolved in ultrapure water, uniformly mixed, and the obtained solution is filtered by a filter membrane and then directly detected by a high performance liquid chromatography evaporative light scattering detector.
As an embodiment of the present invention, the volume of water added in the above-mentioned preparation of the acacia honey sample solution is 3-5 times of the mass of the acacia honey sample. The pretreatment method of the honey sample can be as follows: taking 1g of acacia honey sample, adding 3 mL of ultrapure water, carrying out vortex, fixing the volume to 5mL, filtering with a 0.22 mu m nylon filter membrane, and carrying out sample injection.
The invention has the beneficial effects that: the invention discovers for the first time that the content change of the turanose in the maturation process of the acacia honey has obvious characteristics, and determines that the content of the turanose is more than or equal to 0.5 percent and can be used as a judgment standard of the mature acacia honey for identifying the mature acacia honey and the immature acacia honey and determining the maturity of the mature acacia honey.
The invention develops a method for identifying the maturity of acacia honey by taking turanose as a characteristic standard substance, and the method adopts a high performance liquid chromatography evaporation light scattering detector to detect turanose in acacia honey samples, has higher specificity and sensitivity, and can reach the detection limit of 0.1% for turanose. The invention further optimizes key condition parameters detected by the high performance liquid chromatography evaporative light scattering detector, and improves the accuracy of detecting the turanose in the acacia honey sample.
The method for identifying the maturity of the acacia honey has the characteristics of simple operation, high efficiency, low cost and the like, has reliable and stable detection result, high judgment degree and convenient popularization and application, provides an effective method for identifying the mature acacia honey, has certain guiding significance for the formulation of related industries or national standards of high-quality acacia honey, and has important significance for protecting the legal rights and interests of honey consumers and maintaining the healthy development of the honey consumption industry.
Drawings
FIG. 1 is a chromatogram of acacia honey of different ripeness levels in example 1 of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents and the like used are commercially available unless otherwise specified. Wherein, the used part of instruments and reagents are as follows: high performance liquid chromatography evaporative light scattering detector, Agilent Technologies, usa; electronic analytical balance (PL 203), mettleteledo, germany; ultra pure water machines (Milli-Q Gradient), Millipore Inc. of USA; vortexer (G560E), Scientific Industries, USA.
Example l determination of the content of turanose in Robinia pseudoacacia Honey of different maturity
1. Sample source: in 2019, 2020 and 2021, the acacia honey samples are collected in a plurality of different bee farms of Yanan Shaanxi and the three gorges of Henan (the main production area of acacia honey) for brewing by bees for 1 day (1 d), 3 days (3 d), 5 days (5 d), 7 days (7 d), 9 days (9 d), 11 days (11 d) and 13 days (13 d). For samples on different brewing days, 3 per bee field were taken and the brewing time and honey comb capping rate were recorded. Wherein, the collected samples of 1d-5d are manually concentrated to control the moisture content within the range of 18-21%, and the collected samples of 7d-13d are required to be measured for the moisture content, the moisture content is 21% or less, and the requirement of sealing the honey comb is more than or equal to 75%.
Information on specific acacia honey samples is shown in tables 1 and 2. And (3) performing conventional quality index measurement and pollen identification on all the acacia honey samples, wherein the results show that all the samples accord with the attribute characteristics of the corresponding acacia honey.
And (4) carrying out the content detection of turanose on all collected acacia honey samples.
2. Sample pretreatment: adding 3 mL of ultrapure water into 1g of the acacia honey sample, carrying out vortex, diluting the sample to a volume of 5mL by using water, filtering the sample by using a 0.22 mu m nylon filter membrane, and introducing the sample.
3. Setting the instrument conditions:
(1) conditions of liquid chromatography
A chromatographic column: agilent Hi-Plex Pb, USP L19, 4.0X 250 mm;
column temperature: 70 ℃;
sample introduction amount: 50 muL;
mobile phase: ultrapure water;
elution conditions: isocratic elution;
flow rate: 0.6 mL/min.
(2) Evaporative light scattering detector conditions:
atomization temperature: 90 ℃;
evaporation temperature: 60 ℃;
flow rate of carrier gas: 1.2 SLM;
collecting time periods: collecting for 0-9min (to avoid interference of high content fructose and glucose in Mel), and collecting data for 9-15 min.
4. Drawing a standard curve: preparing a turanose standard substance with the concentration of 0.02%, 0.1%, 0.2%, 0.5%, 1.0%, 2.0% and 5.0%, and drawing a standard curve by calculating the logarithm of the concentration value (the base logarithm of 10) and the logarithm of the response value.
5. Detecting the content of turanose in the acacia honey sample: and (3) making a standard curve according to the linear relation between the content of the turanose and the peak area, and calculating the content according to the standard curve and the peak area of the turanose detected in the acacia honey sample.
Statistics shows that the content of turanose in the acacia honey samples with different maturity is shown in tables 1 and 2, according to the detection results, the content of turanose in the acacia honey samples is more than or equal to 0.5%, the acacia honey can be judged to be mature acacia honey, the result is matched with the result in actual sampling, the condition of the mature acacia honey is met, namely the acacia honey is brewed in a honeycomb for at least 7 days, and the capping rate is more than or equal to 75%. The content of turanose in the acacia honey sample is less than 0.5% and not more than 0.3%, and the acacia honey can be judged to be semi-mature acacia honey, and is brewed in honeycomb for more than 3 days and not more than 5 days, and the capping rate is 30% -70%. The content of turanose in the acacia honey sample is less than 0.3%, and the acacia honey can be judged to be immature acacia honey (1-3d samples, basically without a cover).
The detection patterns of acacia honey with different maturity are shown in figure 1.
TABLE 1 Songaria content (%) of Meadori and Honey comb capping rate (%) in Acacia honey samples of different years and different maturation days in Yanan Shaanxi region (random sampling in bee field of 3 different regions, 1d-13d samples, 3 samples per sample, 63 samples per year, 189 samples per year)
TABLE 2 content (%) of turanose and percent (%) of honey comb cover in acacia honey samples of the three gorges of the Henan province, different years and different days of maturity (3 different regions, random sampling in bee fields of each region, 1d-13d samples, 3 samples per sample, 63 samples per year, 189 samples per year)
Example 2 identification of commercially available Robinia pseudoacacia Honey with turanose as a characteristic marker
1. Sample source
A total of 18 honey samples of various grades or brands labeled acacia honey were purchased from the market, and all samples were subjected to pollen examination to confirm that they were acacia honey.
2. Sample pretreatment: adding 3 mL of ultrapure water into 1g of the acacia honey sample, carrying out vortex, diluting to 5.0mL with water, filtering with a 0.22 mu m nylon filter membrane, and carrying out sample injection.
3. Setting the instrument conditions:
(1) conditions of liquid chromatography
A chromatographic column: agilent Hi-Plex Pb, USP L19, 4.0X 250 mm;
column temperature: 70 ℃;
sample introduction amount: 50 muL;
mobile phase: ultrapure water;
elution conditions: isocratic elution;
flow rate: 0.6 ml/min.
(2) Evaporative light scattering detector conditions:
atomization temperature: 90 ℃;
evaporation temperature: 60 ℃;
flow rate of carrier gas: 1.2 SLM.
4. Drawing a standard curve: preparing a turanose standard substance with the concentration of 0.02%, 0.1%, 0.2%, 0.5%, 1.0%, 2.0% and 5.0%, and drawing a standard curve by calculating the logarithm of the concentration value (the base logarithm of 10) and the logarithm of the response value.
5. Detecting the content of turanose in the acacia honey sample: and (3) making a standard curve according to the linear relation between the content of the turanose and the peak area, and calculating the content according to the standard curve and the peak area of the turanose detected in the acacia honey sample.
The results are shown in Table 3.
TABLE 3 content determination of turanose in Sophora japonica Honey by spot inspection on the market
The detection results show that the content of turanose in 7 samples is greater than 0.5%, the samples are judged to be mature acacia honey, and according to the sample traceability information, the samples can be confirmed to come from an authentication enterprise producing the mature acacia honey, which shows that the maturity identification method provided by the invention has high judgment accuracy. Wherein, the content of turanose in 4 samples is between 0.3% and 0.5%, and the samples are judged to be semi-mature acacia honey, and the content of turanose in 7 samples is less than 0.3%, and the samples are judged to be immature acacia honey. The results prove that the identification method can effectively identify the maturity of the acacia honey, can be used for grading the maturity of the acacia honey commodity honey, and realizes different pricing of the acacia honey according to the maturity.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (4)
1. A method for identifying the maturity of acacia honey is characterized in that an acacia honey sample is detected by using a high performance liquid chromatography evaporative light scattering detector and taking turanose as a characteristic marker, if the content of turanose in the acacia honey sample to be identified is more than or equal to 0.5%, the acacia honey sample to be identified is judged to be mature acacia honey, if the content of turanose in the acacia honey sample to be identified is more than or equal to 0.3% and less than 0.5%, the acacia honey sample to be identified is judged to be semi-immature acacia honey, and if the content of turanose in the acacia honey sample to be identified is less than 0.3%, the acacia honey sample to be identified is judged to be immature acacia honey;
the mature acacia honey is brewed in the honeycomb for at least 7 days, and the sealing cover of the honey comb is more than or equal to 75 percent;
the semi-immature acacia honey is brewed in a honeycomb for more than 3 days and less than or equal to 5 days, and the honey comb is covered by 30-70 percent;
the immature honey is brewed in honeycomb for 0-3 days, and the sealing cover of honey comb is less than or equal to 10%;
the liquid phase conditions detected by the high performance liquid chromatography evaporative light scattering detector are as follows: the method adopts Hi-Plex Pb, USP L19 chromatographic column, the column temperature is 68-72 ℃, water is used as mobile phase, and the elution method is isocratic elution.
2. The method for discriminating the maturity of acacia honey according to claim 1, wherein the flow rate of the mobile phase is 0.5-0.7mL/min, and the sample amount is 45-55 μ L.
3. The method for identifying the maturity of acacia honey according to claim 1, wherein the evaporative light scattering detector conditions detected by the high performance liquid chromatography evaporative light scattering detector are as follows: the atomization temperature was 90 ℃, the evaporation temperature was 60 ℃ and the carrier gas flow rate was 1.2 SLM.
4. The method for identifying the maturity of acacia honey as claimed in any one of claims 1 to 3, further comprising the step of pretreating an acacia honey sample before detecting by a high performance liquid chromatography evaporative light scattering detector, wherein the pretreatment comprises: dissolving the acacia honey sample in water, and filtering.
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| CN202111390505.XA CN113820434B (en) | 2021-11-23 | 2021-11-23 | Method for identifying maturity of acacia honey |
| US18/566,501 US20240255476A1 (en) | 2021-11-23 | 2022-11-22 | Identification method of maturity of acacia honey |
| JP2023553219A JP2024518867A (en) | 2021-11-23 | 2022-11-22 | How to Identify the Ripeness of Acacia Honey |
| PCT/CN2022/133567 WO2023093731A1 (en) | 2021-11-23 | 2022-11-22 | Method for identifying degree of maturity of acacia honey |
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| WO2014171767A1 (en) * | 2013-04-17 | 2014-10-23 | 주식회사 제놀루션 | Method for determining authenticity of honey using dna detection |
| CN104749290A (en) * | 2013-12-26 | 2015-07-01 | 南京工业大学 | High performance liquid chromatography determination method for identifying starch syrup adulteration in honey |
| CN105572237A (en) * | 2014-10-11 | 2016-05-11 | 天津中发蜂业科技发展有限公司 | High performance liquid chromatographic method for rapid quantitative assessment of honey quality |
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Non-Patent Citations (1)
| Title |
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| From Robinia pseudoacacia L. nectar to Acacia monofloral honey: biochemical changes and variation of biological properties;Angelo Gismondi et al.;《Society of Chemical Industry》;20180210;第98卷;第4312-4322页 * |
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